HCID 178478629、化合物 → HCID 178528074、化合物

HRID 411781ノート

反応式

HRID 411781 の反応式
[C:1]1([Li])[CH:16]=[CH:15][CH:14]=[C:13]2[C:2]=1[CH:3]=[C:4]1[C:12]3[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=3[N:6]=[C:5]12.[Cl-].[Cl-].[Cl-].C1([Zr+3:26])C=CC=C1>C1(C)C=CC=CC=1.C(OCC)C>[C:1]1([Zr:26])[CH:16]=[CH:15][CH:14]=[C:13]2[C:2]=1[CH:3]=[C:4]1[C:12]3[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=3[N:6]=[C:5]12

参加物

5

反応物 2

HCID 178478629HCID 178478629、化合物HCID 178506658HCID 178506658、化合物

生成物 1

HCID 178528074HCID 178528074、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒2 回HCID 3283Diethyl Ether溶媒2 回

実験手順

A sample of the indeno[1 2-b]indolyl lithium salt produced above (10 g, 42 mmol) is dissolved in toluene (95 mL) to produce an orange slurry. Diethyl ether (35 mL) is added slowly to give an orange solution. This solution is added over 15 min. at room temperature with stirring to a slurry of cyclopentadienylzirconium trichloride (11 g, 42 mmol) in toluene (190 mL) and diethyl ether (190 mL). The mixture turns deep red and is kept at room temperature overnight. The slurry is filtered to recover a red solid, which is washed with toluene (200 mL) and dried under vacuum. Yield of complex 10: 16.5 g. The 1H NMR spectrum is consistent with the proposed structure:

後処理

  1. customto produce an orange slurry
  2. customto give an orange solution
  3. additionThis solution is added over 15 min. at room temperature
  4. filtrationThe slurry is filtered
  5. customto recover a red solid, which
  6. washis washed with toluene (200 mL)
  7. customdried under vacuum

出典と根拠

ORDレコード
ord-7c5930c9bdd44d4aa67a504df3453fe2
出典データセット
uspto-grants-2003_05
特許番号
US06559251B1

反応ノート

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